Fractionation



E. F. yNELSON FRACTIONATION 'Nom 13, 1945.

Filed Jan.- 51, 1944 Patentecl Nov. 13, 1945 f Y FRAc'rIoNA'rIoN Edwin F. Nelson, Chicago, Ill., assignor. to `Uni-V versal Oil Products Company,l Chicago,l Ill., a corporation of Delaware Application January 31, 1944, serial N0.`520,578

s claims. (criss-94) I'his invention relates to an improved method oi' separating close boiling multi-component fluids, and more particularly to the separation of normally liquid or gaseous hydrocarbons, from a mixture containing two or more fractions of different boiling materials.

The present trend in the petroleum rening industry is toward the synthesis and recovery of relatively pure hydrocarbons. In many instances the recovery of pure hydrocarbons from a mixture of varying boiling point materials is not readily accomplished in conventional systems.

The present invention offers a simple and relatively stable system yfor the separation of relatively close boiling fluids, for-example, hydrocarbons' either normally liquid or normally gaseous. s

Conventional fractionation systems are operated on the basis of maintaining substantially constant operating pressures and substantially constant temperatures. Of course there necessarily must be a temperature gradient from low atthe top of the column to high at the bottom in order to maintain a separation of different boiling fractions; The temperature differential in the column from top to bottom is dependent upon several different factors including thev boiling range of the material being treated. -In general, by means of automatic temperature control an endeavor is made to hold-the temperature at one point in the column substantially constant. This becomes diilicult to accomplish as the differences in boiling range of the fractions decreases as extremely'small changes in either temperature or pressure appreciably changes the purity of the desired products.

The present invention by controlling fractionation without temperature control eliminates some of the difficulties which have been encountered in conventional fractionating systems.

Briefly, the present invention comprises a fractionating system in which fractionation is controlled by a proportionationv of the charging stream into definite lfractions of high and low boiling materials. By charging to the column a substantially constant rate of feed of `substan- I tially uniform quality. and controlling vaporization in the column to maintain a substantially constant quantity of liquid therein, if from the bottom of the column a relatively high boiling fraction of substantially uniform quality material corresponding to a predetermined vportion of the charge is Withdrawn continuously, an overhead product of a substantially uniform quantity and quality will result.

By withdrawing from the bottom of the column a greater or lesser quantity of material than the yhigher boiling component that is present in the charge, it is possible to obtain a bottoms product containing more or less of the lower boiling ma'- terial present in the charge. The degree of separation, of course, will beA dependent to" a large 1 bottom of the column is greater than the proportion of 'higher boiling material Awhichis present in the feed to the column.'

` The invention can bestbe described and rex plained in conjunction with the accompanying diagrammatic drawing which'represents an elevational view of one specific form ofapparatus in which the improved process herein provided may be conducted.

Referring to the drawing, charging material is supplied by means of line I and valve 2 to surge or storage tank 3. This vessel should be oi such a size that variations in the proportions of different boiling materials suppliedthrough line I are substantially equalized and a rmaterial oi fairly uniform `quality is withdrawn through line 4 andvalve -5 lby pump 6. From pump 6 the charging material is directed through valve 'I and line 8 into heat exchanger 9. In heat exchanger 9 the charging material is heated to the desired temperature by means of a suitable heating medium introduced to and withdrawn from the heat exchanger by means of lines I0 and I I and valves I2 and I3, respectively. After passing through heat exchanger 9 the charging materialis directed through an orice flange `I4 and a flow control valve I5 after which it passes into fractionating column 2I. Orice I4 and flow control valve I5 operate in conjunction with a suitable flow control instrument I 6. by means of which Athe pressure differential across orifice I4 communicated to instrument IS by means of linesk I8 and I9 is converted to impulses transmitted Afrom instrument I6 by means of conduit 20 Vto valve I5 and which function to open or close the latter in 'response to decreases or increases in the flow 1 or iiuid through line 8.

form quality.

Fractionating column 2| may be'any of the conventional types now in common use containing suitable packing or bubble trays not shown. Heat is supplied to `the lower portion of the column by means of reboiler 22, which communi- Cates with the column through conduits 23 and y y Thevaporous materials from the top 24. Heat is supplied to the reboiler by means of a suitable heat convective fluid suchv as steam introduced through -line 25, and control valve 26 and in case steam is employed the condensate is withdrawn froml the reboiler by means of line 21, trap 28, and valve 29. The bottoms product from the fractionator is withdrawn at a substantially constant rate through line 30, orifice 3l. and valve 32. Orifice 3l and valve 32 operate in conjunction with a suitable flow control Airi-V strument 33, similar to instrument I6. Instrument 33 operates to vary the setting of valve `32 Ain response to differentials in pressure across orifice 3l, similar to the operation of instrument i6;

In desired instances it ispossible to automatically control the proportionation of thecolumn. That is, by interconnecting instruments i6 and product containing the higher boiling of the two components, the flow control instrument for the bottom product would be set at such a rate that less than 50% of the charge would be withdrawn therethrough. The exact difference between percentage of the higher boiling component in the vcharge and the percentage of the charge which is withdrawn from the bottoms which will give the desired quality of product will be dependent upon vthe efficiency of the fractionating column.

By withdrawing a regulated proportion of the charge as a bottom product, maintaining the charge at a substantially uniform rate and of a' substantially constant quality, and maintaining the liquid level in the bottom of the column and the ,reflux ratesubstantially constant, the over- 33 in a manner which is well known tothe art so that instrument I6 operates toreset instru- -ment 33,. it is'possible to automatically. regulate the quantity ofbottoms withdrawn to maintain it at a rate correspondingto a definite proportion of the feed. i

The flow of heating fluid'r intoreboiler 22 is controlled in response to variationsinthe liquid level in fractionating `column 2| as indicatedby the broken ,line y34. vThis control of heating fluid is accomplished by means of control valve'26 and asuitablecOnVentiOnal type of liquid level-control instrument 35. The flow control instrument ,may be of the external float cage type as illus- :trated or .when desired an internal float may be utilized. The variations in the positionof the i. float function to Vary air pressure. in line 36.. l which in turn functions to .vary the opening-lor closing of .valve` 26. f With an increase of V.the ,liquidlevel in the column the instrument is so arvranged that control valve 26 will open thus .,alf lowing more heating fluid to enter theY reboiler and cause a more rapid vaporization of the liquid in the bottom of the fractionating column. With alowering of the liquidflevel in the column, con-V trol instrument 35 and valve 26 will function to `decrease the heatingmedium suppliedjtoj the re=l vboilerthus reducing the degree of vaporization of the liquid in the column` y column areA withdrawn through line 3lL and pass through condenser 38, the condensed materials being collected fin accumulator 39. A portion of this condensed `material `is withdrawn through oi.'v the o head product will also be of a substantially con-` stant quality and at a substantially uniform rate.

I claim as my invention:

said material at asubstantially uniform rate into ka fractionating column, withdrawing liquid .at a.

substantially uniform ratev from the bottom of said fractionating column, removing vaporous materialoverhead ,from said column. cooling said Y vaporous material and supplying a portion of the A, resultant condensate at a substantially uniform rate'tothe top o f said fractionating column as reflux therefor, and supplying heat to the bottomy of said columnat a rate varying in response to changes'in the liquid level in the bottom of said column. said rate being increased with increasing liquidleveland decreased with decreasing liquid linev 4U "and, directed by-.means of pump.-4i'.1 1 through line 42, orifice 43, and control valve-344 `into the upper portion ofl the fractionating col'-v umn to serve as reflux for the column. Orifice:

43 and control valve `44- are interconnected with a suitable iiow control instrument 45 and'function to maintain` the iiow` of reflux througlrline 42 at asubstantially constant rate.l Theoperation of 1nstrument45 is similar to that described for` instruments IB and 33.5 ABy varying thesetvting of instrument 45 it is possible to maintain any reflux ratiothat may be desired.

The overhead'fproduct from, the -fra-ctionating `column 1s withdrawn from accumulator 39 1 2A method of fractionatingA a multi-component fluid material .which comprises introducing said material at a substantially uniform rate into a fractionating column, withdrawing liquid at a substantially uniform rate from the bottom of saidfractionatingcolumn, removing vaporous material overhead from said fractionating column; cooling ysaid` vaporous material, and supply- "ing av portionpofthe resultant condensate at a substantially luniform rate tothe top of said fractionating column as .reflux therefor, and con-` trolling the degree 'ofvaporization in said fractionating column by increasing the heat supplied Vto the bottomofsaid column in response to increases in the liquid level in the bottom of said -column and decreasing the heat supplied to the bottom of the column-in response to vdecreases y. in said liquid level.v l

3. A method of separating narrow boiling range hydrocarbons into low and high boiling fractions` which comprises'introducing said hydrocarbons at a substantiallyk uniform rate into a fractionatingA column, withdrawing a liquid fraction at a substantially uniform rate from the bottom of said fractionating column as said high boiling fraction, removingk vaporous material overhead y from, said column as said low boiling fraction,

If in this case, for

cooling said vaporous material and supplying a portion of the resultant condensate at a substantially `uniform rate to the top of said fractionating "column as reflux therefor, and controlling the 4degree of vaporization in said fractionatlng column by-increasng the heat supplied to the bottom of said column in response to increases in the liquid level in the bottom of said column and decreasing the heatsupplied to the bottom of the column in response to decreases in said liquid level. f EDWIN F. NELSON.`

l. A method of fractionating a multi-compor-y v nent-fluid material which comprises introducing 

